CN104126027A - Multi-chambered acoustic sensor for determining gas composition - Google Patents

Multi-chambered acoustic sensor for determining gas composition Download PDF

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Publication number
CN104126027A
CN104126027A CN201280057412.8A CN201280057412A CN104126027A CN 104126027 A CN104126027 A CN 104126027A CN 201280057412 A CN201280057412 A CN 201280057412A CN 104126027 A CN104126027 A CN 104126027A
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sensor
acoustic
gas
chamber
gases
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CN104126027B (en
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A.瓦杰德
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Inficon Inc
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Inficon Inc
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01HMEASUREMENT OF MECHANICAL VIBRATIONS OR ULTRASONIC, SONIC OR INFRASONIC WAVES
    • G01H3/00Measuring characteristics of vibrations by using a detector in a fluid
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01HMEASUREMENT OF MECHANICAL VIBRATIONS OR ULTRASONIC, SONIC OR INFRASONIC WAVES
    • G01H5/00Measuring propagation velocity of ultrasonic, sonic or infrasonic waves, e.g. of pressure waves
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N29/00Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object
    • G01N29/02Analysing fluids
    • G01N29/024Analysing fluids by measuring propagation velocity or propagation time of acoustic waves
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N29/00Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object
    • G01N29/02Analysing fluids
    • G01N29/036Analysing fluids by measuring frequency or resonance of acoustic waves

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  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Acoustics & Sound (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analyzing Materials By The Use Of Ultrasonic Waves (AREA)

Abstract

A sound velocity sensor is defined by a hermetic multi-chambered enclosure for containing flowing gases and mixtures of gases. The contained flowing gases are acoustically excited and the acoustic energy is measured over a fixed distance between a first sending end of the enclosure and a receiving end. The speed of sound of the gases are determined by comparing the energy transmitted through the flowing gases at various frequencies so as to precisely determine the resonant frequency of the gases flowing through the enclosure. In accordance with the present design, the chambers of the enclosure include internal transition shapes therebetween for optimizing the transmission of acoustic energy through the flowing gases and also enhancing one or more additional resonant modes at higher useful frequencies. The transition shapes used in connection with the sensor can be at least one of parabolic, hyperbolic, linear and exponential in nature.

Description

For determining the multicell acoustic sensor of gaseous fraction
The cross reference of related application
The application requires the right of priority of the u.s. patent application serial number 61/562,661 of submitting on November 22nd, 2011 according to the relevant trifle of the 119th section of the 35th article of United States Code, and this application is integrally merged in by reference.Also to U.S. Patent number 6,482,649 and 5,768,937 carry out reference in this article, and wherein, the full content of each one is incorporated into herein by reference.
Technical field
The application relates generally to processing substrate field, and relates more specifically to multicell acoustic transducer or be used to determine and control the unit with respect to the gaseous fraction of various chemical vapor depositions (CVD) technique.
background technology and summary of the invention
Chemical vapor deposition (CVD) technique is widely used for the layer of the various thickness of growing metal, semi-conductor, dielectric medium etc.Typical case's CVD technique requires the growth material of expecting to be attached to ligand or volatility adducts conventionally, and it allows the expectation species in vapour phase to be transported to (multiple) substrate and to be arranged in the reaction zone of reactor wherein.This complicated molecule is commonly called precursor.Different materials has different front body structures.
Once in reaction zone, a part for volatile precursor compound is decomposed, make volatile precursor compound separate with non-volatile part and the solid deposits of expectation is left on (multiple) substrate.Conventionally, decomposition reaction is that heat drives; That is, substrate is heated to sufficiently high temperature, so that in the time of volatile compound contact substrate, makes enough energy can be used for interrupting existing connection the between volatility ligand or adducts and expectation atom.The atom of expecting is still deposited on substrate, and then the volatility part of precursor gases is discharged from from reactor by outlet port.Although heat energy is means for driving CVD reaction, exists can be used in and scatter suitably other process mechanism of deposition.
As being entitled as: the U.S. Patent number 6 of Acoustic sensor for in-line continuous monitoring of gasses, 482, described in 649, applicant had previously determined for controlling such as MOCVD(Organometallic Chemistry gas deposition) precursor delivery of CVD reactor reactor determine the component of binary gas mixture to determine the supply of at least one acoustic elements in the Gas controller of efficiency of reactor.This type of reactor is used to for example manufacture for the object of opticfiber communication the object of compound semiconductor device.Calculating flows through the speed of the sound of the gas of device, and wherein device operates in mode of resonance.Determine according to the speed of the resonant frequency of measuring and sound, can determine import and outlet (discharge) gaseous fraction.Utilize the principle of describing in the patent of ' 649, after this applicant has made the system commercialization being mentioned with trade(brand)name Composer Gas Controller.
At present, there is the recovery of the interest to MOCVD reactor, for example, for high-brightness LED manufacturing process.Although the Composer device of current design due to the resolving power of its measurement and repeatable and very remarkable in its epoch, exists current device not to be designed to particularly the new challenge that will tackle at present.For example, the TMIn precursor of being carried by hydrogen carrier gas is typical in the past.But at present, using nitrogen is maximum challenge as the conveying of the Cp2Mg of carrier gas.Fig. 1 has described each in foregoing example with graphics mode.(in regard to same) equally, the molecular weight ratio of precursor and carrier gas is to determine the greatest factor of theoretical resolution aspect of device, as by reference by described in ' 649 patent above being integrally incorporated herein.And the transition from hydrogen carrier gas to nitrogen carrier gas particularly, this key factor is reduced to 1/14th therefore.
But, determine and can overcome significantly this shortcoming by the various amendments to acoustic resonator, as described herein, it can operate acoustic resonator and can not change widely its overall dimension under upper frequency now.
Business sells acoustic transducer and specifies that for introducing the micropkonic constraint of acoustic energy and the restriction of isolation diaphragm device should operate at approximately 500 Hz for the purpose of practicality to the range of frequency of approximately 5000 Hz.In the compound resonator in multiple chambeies that comprises different sizes (such as the formerly U.S. Patent number 6,482 the applicant, those described in 649), can allow resonant frequency is not to be correlated with harmonically.For example, in newly-designed acoustic resonator (will elaborate below), in theoretical resonant frequency nitrogen at room temperature, be 1208 Hz, 3948 Hz, 6827 Hz, 10161 Hz etc.Although resonant frequency is different in different gas, but frequency ratio is still identical, and is determined by the geometrical shape of compound resonator.
Therefore, a kind of sonic sensor is provided in this article, this sensor comprise sealing multicell shell for comprising flowing gas and gaseous mixture, for excitation on acoustics comprise flowing gas device and for measuring the device of the acoustic energy transmitting in the fixed range between the first sending end and its receiving end of described shell.Determine the speed of the sound of gas by the energy relatively transmitting by flowing gas under various frequencies, thereby accurately determine the resonant frequency of the gas that flows through shell.According to the design, the chamber of shell be included between it for optimizing acoustic energy by the transmission of flowing gas and for strengthening the inner transition shape of the one or more additional resonance patterns under higher useful frequency.
The intermediate shape using in conjunction with sonic sensor as herein described can be suitably shape continuously of at least one in para-curve, hyperbolic line, straight line and index curve or other in fact, so that the transmission of acoustic energy the acoustic impedance loss in point chamber enclosure of sensor is minimized.
Can produce therein and hold facile transmission, receiving transducer and isolation diaphragm and this device and fail to have in the scope of significant self-resonance pattern by the attainable additional resonance pattern of current described sensor.
According to a preferred styles, first-harmonic resonance frequency and additional resonant frequencies are between approximately 400 Hz and about 6000Hz.
Be preferably accurate level arbitrarily by sensor housing and the temperature control by its mobile gas.
Definite resonant frequency can be used to for example to derive the component of the binary gas mixture using in the reactor such as utilizing the reactor of MOCVD technique.
Advantageously, sensor improves the speed that the sound of the acquisition that has strengthened the definite stability of resonant frequency and susceptibility and obtain calculates as discussed above.
According to the following detailed description that should read in conjunction with the accompanying drawings, these and other feature and advantage will be apparent.
Brief description of the drawings
Fig. 1 is the diagrammatic representation relevant to frequency displacement contrast binary gas component, and it relates to the specific precursor that uses various carrier gas combinations;
Fig. 2 is the diagrammatic representation that uses the acoustic resonator resonance peak that combination creates for specific gas of making according to an embodiment;
Fig. 3 is according to the expression of the stability of the acoustic resonator of an one embodiment;
Fig. 4 is the partial cross section front view of prior art acoustic resonator;
Fig. 5 is the partial cross section front view according to the acoustic resonator of exemplary embodiment; And
Fig. 6 illustrates the comparative frequency displacement causing according to the specific precursor gases due in hydrogen and nitrogen carrier gas in two of exemplary embodiment modes of resonance, wherein makes sensitivity become four times by operation in the second mode of resonance.
Embodiment
Below describe and relate to for the example acoustic resonator in the treatment reactor of chemical vapor deposition (CVD) or other form (being also referred to as from start to finish " acoustic elements " or " acoustics (velocity of sound) sensor ").It is evident that other suitable amendment and modification are possible in those of ordinary skill in the art's level.In addition, spread all over this description and pass through U.S. Patent number 6,482,649 and 5,768,937 reference comes with reference to the multiple background characteristics about CVD reactor assembly, and this patent is each to be integrally incorporated to by reference.
First Fig. 4 is carried out to reference herein, described the prior art composite acoustic resonator 30 that uses in combination with CVD or other similar process reactor (not shown), as at U.S. Patent number 6,482, be also described in 649.Be understood that integral reactor system comprises multiple parts, it comprises various sensors, reactor itself, bubbler chamber etc.Just about the each aspect in these parts, ' 649 patent is carried out to reference in this article, wherein, the focus of this discussion is that resonator or the acoustic elements to therewith using carried out.
The acoustic resonator 30 of utilizing is limited by housing 34, and it is preferably made up of metallic substance and comprises combination and form multiple adjacent acoustic chamber 38,40,44 of resonator chamber 48.Provide drive unit such as driving speaker (not shown) to send acoustical signal by the gas that flows through acoustic cavity 38,40,44 at sending end 52 places of resonator 30, cause that gas flows through resonator chamber 48 via suitable import and outlet port (not shown), and wherein, acoustic energy is arranged on the reception speaker (not shown) reception at receiving end 56 places that connect of resonator 30.Details about driving and receiving trap/speaker, gas feed and outlet port and correlated characteristic is provided in ' 649 patent being previously incorporated to.
In this prior art compound resonator 30, acoustic cavity 38,40,44 is each to be limited by different sections, chamber is connected to each other to limit overall resonance device chamber 48 by corresponding discontinuous end segment 56,60,62,64, wherein each acoustic cavity is limited by fixed diameter and section, and wherein, the diameter of acoustic cavity 40 is more much smaller than the diameter in adjacent acoustic chamber 38,44.In operation, cause that binary gas mixture (for example, precursor and carrier gas) flow to acoustic cavity 38 from gas feed port, wherein further cause that gas flow passes through the each pneumatic outlet port that arrives in adjacent acoustic chamber 42,44.Apply acoustic energy at the sending end place of housing 34 and by the acoustic cavity that limits resonator chamber 48.At this sensing housing and the temperature of flowing gas for example control it, for accurate level (, 0.1 degree Celsius) arbitrarily operating period.The acoustic energy obtaining of measuring at the receiving end place of housing 34 provides the instruction of the speed (c) of sound, and then these data are used for determining gaseous fraction, reactor efficiency and other parameter in the mode described in the patent of basis ' 649.
But, due to the mismatch of acoustic impedance two sections (for example determine, locate 56,60 etc.) interface there is transmission loss (the Fundamentals of Acoustics following, L.E.Kinsler, A.R.Frey, A.B.Coppens & J.V.Sanders, Third edition, page-234).The sectional area of known acoustic impedance and element is inversely proportional to.
Can and more preferably between the acoustic cavity that limits shell, create intermediate shape gradually by the transition between the chamber (chamber) of adjustment acoustic resonator minimizes this loss.Fig. 5 has described an exemplary embodiment of acoustic resonator 80, and it is that with the similar of pattern above resonator is by having the metal shell 84 in three (3) adjacent acoustic chambeies 86,88,90 and receiving the sending end 91 of the acoustic energy drive unit such as speaker (not shown) and comprise that the receiving end 93 that connects of the compatible apparatus for receiving the acoustic energy driving by resonator 80 limits.But according to the design, acoustic cavity 86,90 is not provided constant section, wherein, the diameter of acoustic cavity 86 along endways section 94 places start the parabolic outlines 100(profile towards less adjacent acoustic chamber 88) inwardly phase down.The internal diameter of acoustic cavity 88 is substantially constant in its axial length, and wherein, the diameter in adjacent acoustic chamber 90 outwards increases, and also, along the same parabolic outlines 100 of acoustic cavity 86, extends to end segment 98.Parabolic outlines 100 provides the transition gradually between acoustic cavity each, and eliminates any discontinuity that trends towards causing by resonator 80 acoustic impedance between it.It should be noted that the para-curve taper using the acoustic cavity interconnection of device described herein is exemplary.Further recognize other on-fixed pattern that can also utilize gradual change taper; For example hyperbolic line, index curve and linear taper are all tested and be verified as and providing useful result aspect the acoustic energy transmission of acoustic impedance loss with minimizing.Net result is the better signal to noise ratio during resonant frequency is measured.
Owing to now providing above-mentioned Geometrical change by the acoustical device of Fig. 5 compared with the prior art device pattern of describing at Fig. 4 place, the rate of air sucked in required (swept volume) of system is reduced.In particular example as herein described, rate of air sucked in required is decreased to below 9 cc from approximately 18 cc.The rate of air sucked in required that minimizing is provided is favourable, because it has shortened the time of response at the unexpected During of flowing gas component.
Using the additional benefits of acoustic resonator described herein design is the enhancing of mode of resonance, and this device can be utilized together with various precursors/carrier gas combination, such as relatively adopting nitrogen as those of carrier gas with hydrogen.For example and use acoustical device as herein described in reactor assembly (such as conventionally by described in the patent of ' 639 and with reference to figure 2), use acoustic resonator 80 as herein described to show the resonance peak of the R134a in nitrogen in the window of 500 Hz to 5000 Hz (component arbitrarily).By applying the actuate signal of continuous frequency conversion (frequency sweep), can advantageously identify multiple resonance peaks.Sometimes, some in peak value are parasitic (spurious), such as the one or more speaker resonance due in gas feed/outlet pipe.Because the frequency ratio of real adjacent peak value will be known, so can easily identify and abandon not and those parasitic peak of pattern-fitting.
Once parasitic peak is dropped, analyze all the other resonance peaks and select there are the highest Q(quality factor) peak value of value is for watch-keeping.Generally speaking, highest frequency peak value has the highest Q value.For example, in the acoustic resonator described herein in the nitrogen under STP, the first peak value appears at approximately 1208 Hz places, and Q=21.Next peak value appears at 3948 Hz places, and Q=72.Therefore, expection the second peak value provides better measurement stability and the roughly sensitivity of better four times compared with the first peak value.Fig. 3 show pure nitrogen gas and the nitrogen that mixes using the R134a of 50 ppm in the typical sensitivity of the acoustical device 80 as example.
For the parts list of Fig. 1-5
30 acoustic resonator
34 housings
38 acoustic cavities
40 acoustic cavities
44 acoustic cavities
52 ends, send
56 ends, receive
58 end segment
60 end segment
62 end segment
64 end segment
80 resonators
84 housings
86 acoustic cavities
88 acoustic cavities
90 acoustic cavities
91 ends, send
93 ends, receive
94 end segment
98 end segment
100 tapers, gradual change (intermediate shape).
Will be appreciated that, in the desired extent of concept described herein, other variants and modifications is possible, it will be apparent for the personnel of enough technology in this area.

Claims (11)

1. a sonic sensor, comprising:
Sealed enclosure, for comprising flowing gas and gaseous mixture, described shell comprises the chamber of multiple interconnection;
For with acoustically excitation comprised flowing gas device; And
For measuring the device of the acoustic energy transmitting in the fixed range between the first sending end and the receiving end of described shell, wherein determine the speed of the sound of gas by the energy relatively transmitting by flowing gas under different frequency, thereby accurately determine the resonant frequency of the gas that flows through described shell, and wherein, the chamber of described shell comprises the inner transition shape between the adjacent chamber for optimizing acoustic energy at least one additional resonance pattern under higher useful frequency by the transmission of flowing gas enhancing.
2. sensor as described in claim 1, wherein, described intermediate shape is by being configured to be convenient to the transmission of acoustic energy and the minimized continuous shape of acoustic impedance loss in described sensor being limited.
3. sensor as described in claim 1, wherein, described intermediate shape is hyp.
4. sensor as described in claim 1, wherein, described intermediate shape is index curve.
5. sensor as described in claim 1, wherein, described intermediate shape is straight line.
6. sensor as described in claim 1, comprise for by the temperature control of vessel and flowing gas to the accurate device of level arbitrarily.
7. sensor as described in claim 1, wherein, the chamber of described shell is relative to each other different in size.
8. sensor as described in claim 3, wherein,, in such scope, wherein can produce the facile transmission of appearance, receiving transducer and isolation diaphragm and device and fail to have significant self-resonance pattern by the attainable additional resonance pattern of current described sensor.
9. sensor as described in claim 1, wherein, the first-harmonic resonance frequency of described sensor and additional resonant frequencies are between approximately 400 Hz and about 6000Hz.
10. sensor as described in claim 1, wherein, described sensor is configured to for utilizing in the reactor of MOCVD technique, and wherein determined resonant frequency can be for example for deriving the component of the binary gas mixture using at described reactor.
11. 1 kinds for the manufacture of the method for sonic sensor of reactor of utilizing MOCVD technique, and described method comprises the steps:
Provide there is sending end, the shell of receiving end and the multiple linear chambers that arrange between described sending end and described receiving end;
Between described chamber, be provided for optimizing the intermediate shape of acoustic energy transmission.
CN201280057412.8A 2011-11-22 2012-11-21 Multi-chambered acoustic sensor for determining gas composition Active CN104126027B (en)

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US201161562661P 2011-11-22 2011-11-22
US61/562661 2011-11-22
PCT/US2012/066253 WO2013078308A1 (en) 2011-11-22 2012-11-21 Multi-chambered acoustic sensor for determining gas composition

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DE (1) DE112012004853T5 (en)
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CN109490211A (en) * 2018-11-16 2019-03-19 安徽理工大学 A kind of photoacoustic cell with anti-noise function

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GB2519184B (en) 2017-12-06
US20130125622A1 (en) 2013-05-23
GB201408296D0 (en) 2015-04-01
KR20140096285A (en) 2014-08-05
GB2519184A (en) 2015-04-15
CN104126027B (en) 2017-04-12
US9217663B2 (en) 2015-12-22
DE112012004853T5 (en) 2014-08-28
KR101956955B1 (en) 2019-03-11

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